有机化学 ›› 2011, Vol. 31 ›› Issue (06): 824-831. 上一篇    下一篇

研究论文

含1,3,4-噁二唑和1,3,4-噻二唑的硫醚类化合物的合成

武现丽,朱春风,吕志丹,魏成事,廖新成*   

  1. (郑州大学化学系 郑州 450052)
  • 收稿日期:2010-09-10 修回日期:2011-01-10 发布日期:2011-01-21
  • 通讯作者: 廖新成 E-mail:lxc66@zzu.edu.cn

Synthesis of Sulfur Ethers Containing 1,3,4-Oxadiazole and 1,3,4-Thiadiazole

WU Xian-Li, ZHU Chun-Feng, LV Zhi-Dan, WEI Cheng-Shi, LIAO Xin-Cheng   

  1. (Department of Chemistry, Zhengzhou University, Zhengzhou 450052)
  • Received:2010-09-10 Revised:2011-01-10 Published:2011-01-21
  • Contact: Xin-Cheng Liao E-mail:lxc66@zzu.edu.cn

在KOH作用下, 芳甲酰肼1a1e与CS2环化生成5-芳基-2-巯基-1,3,4-噁二唑(2a2e);将2a2e与氯乙酸乙酯反应, 生成2-(5-芳基-1,3,4-噁二唑)硫基乙酸乙酯(3a3e);3a3e肼解得2-(5-苯基-1,3,4-噁二唑-2-硫基)乙酰肼(4a4e);4a4e与芳酰基异硫氰酸酯5a5d反应得到双酰基氨基硫脲衍生物A1A19;A1A19在H2SO4催化下环合得到目标化合物B1B19;目标化合物的结构经IR, 1H NMR, MS, HRMS确证.

关键词: 1,3,4-噁二唑, 1,3,4-噻二唑, 氨基硫脲, 硫醚

5-Aryl-2-mercapto-1,3,4-oxadiazoles (2a2e) have been obtained by the reaction of arylcarboxylic acid hydrazides 1a1e with carbon disulfide in the presence of potassium hydroxide. Then the reaction of compounds 2a2e with ethyl chloroacetate produced 2-(5-aryl-1,3,4-oxadiazol)thio esters (3a3e). The treatment of compounds 3a3e with hydrazine hydrate resulted in the formation of acide hydrazides 4a4e. The biacyl thiosemicarbazide derivatives A1A19 were synthesized by the reaction of corresponding compounds 4a4e with aroyl isothiocyanates 5a5d. The target compounds B1B19 were prepared by cyclization of compouds A1A19 in the presence of CH3OH/H2SO4, and their structures were confirmed by IR, 1H NMR, MS and HRMS techniques.

Key words: 1,3,4-oxadiazole, 1,3,4-thiadiazole, thiosemicarbazide, sulfur ether